High-strength, low-temperature-resistant, low-warp bottom guard plate material and preparation method thereof

By using recycled materials and specific processes to prepare high-strength, low-temperature resistant, and low-warping underbody protection material, the problems of insufficient performance and high cost of existing materials in high and low temperature environments and complex road surfaces have been solved, realizing environmentally friendly and economical material recycling.

CN120904579BActive Publication Date: 2026-02-17QIHE TECH (JILIN) CO LTD
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Patent Information

Application Number
CN202511435484.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-10-09
Publication Date
2026-02-17
Estimated Expiration
2045-10-09

AI Technical Summary

Technical Problem

Existing automotive underbody protection materials cannot simultaneously meet the requirements of high strength, low temperature resistance, and low warpage under high and low temperature environments and complex road conditions. In addition, the materials are costly, have low resource utilization efficiency, and cause serious environmental pollution.

Method used

High-strength, low-temperature resistant, and low-warping bottom protection plate material is prepared by using recycled PP granules, recycled photovoltaic film granules, glass fiber, treated silica, and other additives from the inner tub of a single-cylinder washing machine, through a specific mixing and extrusion granulation process, thereby reducing dependence on virgin petrochemical materials.

Benefits of technology

This has resulted in reduced material costs and carbon emissions. The material maintains good flexibility and strength at low temperatures, reducing product warping and meeting the needs of use in complex environments.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application belongs to the technical field of plastic modification, and relates to a high-strength, low-temperature-resistant and low-warp bottom protection plate material and a preparation method thereof. The method comprises the following steps: taking polypropylene resin particles, toughening agent resin particles, a compatibilizer and black masterbatch into a stirring pot; adding a wetting agent and stirring at 350 RPM; adding a processing aid package and treated silicon dioxide into the stirring pot and stirring at 350 RPM; adding the mixed material into a main feeding loss weight scale; adopting a 40:1 length-diameter ratio, adding chopped glass fibers into the side feeding loss weight scale at the sixth extruder cylinder, setting the discharging amount of the main loss weight scale as 35 kg / hour, setting the discharging amount of the side loss weight scale as 15 kg / hour; starting the main machine with a frequency of 38 Hz, starting the feeding, starting the auxiliary equipment, and performing granulation production. The method can reduce the dependence on virgin petrochemical products and reduce carbon emissions by using regenerated materials, and the prepared material can meet the requirements of high strength, low temperature resistance and low warping.
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Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of plastic modification, and particularly relates to a high-strength, low-temperature-resistant and low-warp underbody shield material and a preparation method thereof. BACKGROUND

[0002] At present, the automobile underbody shield is mainly a polypropylene reinforced material. The automobile can travel in the country or even the whole world and can experience various complex road environments, so that the material has strict requirements on low-temperature resistance, high strength and the like. At present, in order to cope with complex working conditions, the original petrochemical material is basically selected for modification. With the global economic development and population growth, the demand for petrochemical resources is increasing, and the over-consumption of resources leads to serious shortage. Moreover, a large amount of garbage is generated after use, which not only pollutes the environment but also affects the ecological balance and threatens human health. Therefore, resource recycling and reuse are imminent, and how to recycle limited resources is an important environmental protection issue. The development of circular economy industry is the driving force for resource recycling and reuse. The circular economy industry not only reduces the dependence on primary resources, but also creates a new economic growth model. Therefore, it is urgent to develop a method for preparing a high-strength, low-temperature-resistant and low-warp underbody shield material using part of PCR materials.

[0003] The prior art discloses a high-heat-oxidation-resistant environment-friendly recycled polypropylene material and a preparation method thereof. The high-heat-oxidation-resistant environment-friendly recycled polypropylene material is prepared from the following raw materials in percentage by weight: waste polypropylene 50-80%, inorganic filler 0-30%, elastomer POE 5-20%, interface modifier 0.5-5%, coupling agent 0.1-2%, antioxidant 0.1-2%, and after mixing, melt extrusion, granulation, drying treatment and the like. Although the recycled polypropylene material obtained by the method has high room temperature toughness and heat-oxidation resistance, it ignores the driving environment of the automobile, and needs to meet the relatively complex high and low temperature and the potholed road surface covered with gravel. Moreover, the method does not list the low-temperature resistance and the ball drop impact test of the material, and the rigidity of the material is poorer than that of the glass fiber filled material, so that the material cannot completely protect the internal parts when encountering potholed road surface and is prone to damage the internal parts.

[0004] The prior art also discloses a polypropylene composite material for automobile underbody shields prepared by using LFT-D technology, comprising 75-90 parts by weight of high melt index polypropylene, 2-15 parts by weight of a compatibilizer, 0.5-5 parts by weight of a flow modifier, 0.5-3 parts by weight of high-mesh talcum powder, 0.2-2 parts by weight of a compounded antioxidant system and 0.2-2 parts by weight of a lubricant. The composite material has the characteristics of high rigidity and high flow, and has good processing performance and heat aging resistance, and prevents fiber floating and glass fiber agglomeration. However, when high-flow polypropylene is combined with a flow modifier, the molecular chain length and regularity are further reduced, resulting in a large difference in the uniformity of the material crystallization. At the same time, when the material is prepared by injection molding LFT-D technology, glass fiber directional flow occurs, which finally leads to warping of the product. The material matrix uses virgin petrochemical products, the cost is relatively high, and the market acceptance is not high.

[0005] Therefore, it is urgent to develop an underbody shield material which can meet the requirements of low cost, high strength, low temperature resistance and low warping, so as to effectively solve the above problems. SUMMARY

[0006] The purpose of the present application is to provide a high-strength, low-temperature-resistant and low-warp underbody shield material and a preparation method thereof, so as to solve the problems of reducing the cost of underbody shields, realizing low-temperature impact resistance, low warping and material recycling.

[0007] The present application is realized by the following technical solutions:

[0008] A high-strength, low-temperature-resistant and low-warp underbody shield material is prepared from the following raw materials by weight:

[0009] Polypropylene: 51 parts,

[0010] Toughening agent: 8 parts,

[0011] Compatibilizer: 5 parts,

[0012] Glass fiber: 30 parts,

[0013] Treated silicon dioxide: 3 parts,

[0014] Processing aid package: 1 part,

[0015] Wetting agent: 0.5 parts,

[0016] Black masterbatch: 1.5 parts.

[0017] Further, the polypropylene is a single-cylinder washing machine inner barrel PP recycled material particle, and the ash content is less than 0.2%; the toughening agent is a photovoltaic film, which is a four-carbon POE thin film recycled particle prepared after partial crosslinking, and is formed by recycling and granulation after use; the compatibilizer is a granular polypropylene grafted maleic anhydride; the wetting agent is a liquid 10# white oil; and the black masterbatch is a PE carrier color masterbatch with a carbon black content of 35%.

[0018] Further, the glass fiber is a chopped glass fiber.

[0019] Further, the silicon dioxide is a nano material in the form of powder, which is a by-product of sodium silicate formed by manufacturing a capacitor carbon from rice husk, and is finally formed into silicon dioxide powder after treatment, and is treated to form treated silicon dioxide.

[0020] Further, the processing aid package is a powder, which includes an antioxidant and a lubricant; wherein the antioxidant includes antioxidant 1010, antioxidant 3114, antioxidant 168, and antioxidant DSTDP, the content of antioxidant 1010 is 0.15%, the content of antioxidant 3114 is 0.15%, the content of antioxidant 168 is 0.2%, and the content of antioxidant DSTDP is 0.3%; and the content of the lubricant EBS is 0.2%.

[0021] A preparation method of a high-strength, low-temperature-resistant, and low-warp bottom guard plate material, comprising the following steps: weighing polypropylene resin particles, toughening agent resin particles, a compatibilizer, and a black masterbatch into a stirring pot; then, adding a wetting agent, stirring at 350 RPM for 10 minutes; further adding a processing aid package and treated silicon dioxide into the stirring pot, stirring at 350 RPM for 10 minutes; adding the mixed material into a main feeding loss weight scale; using a device with a length-diameter ratio of 40:1, adding chopped glass fibers into a side feeding loss weight scale at the sixth section of the extruder cylinder, setting the discharge amount of the main loss weight scale to 35 kg / hour, and setting the discharge amount of the side loss weight scale to 15 kg / hour; starting the main machine, starting the feeding, starting the auxiliary equipment, and performing granulation production.

[0022] Further, it specifically comprises the following steps:

[0023] A, preparation of treated silicon dioxide:

[0024] A1, first filter the by-products such as sodium silicate formed by manufacturing a capacitor carbon from rice husk, remove impurities, and test the concentration of sodium silicate in the solution;

[0025] A2, introduce the sodium silicate solution into an evaporator, heat the evaporator to boiling of the solution, evaporate the water in the by-products such as sodium silicate, and increase the concentration of sodium silicate; when the concentration of sodium silicate reaches 20%-25%, stop heating and discharge;

[0026] A3, into the reaction pool, open the stirring paddle, speed is 245 RPM, open the heating system, control the material temperature at 80-90℃, through the addition of 16% concentration of hydrochloric acid by the aid of pump, control the overall material PH value at 7.5-8.5, stop adding hydrochloric acid, at this time, the generation of colloidal material, discharge;

[0027] A4, into the dehydration pool, heating temperature 152℃, until the constant weight of the material in the dehydration pool, at this time, the colloidal material is completely decomposed into silicon dioxide, and water is removed in the form of water vapor, finally discharge;

[0028] A5, the material obtained in step A4 enters the rinsing pool, the stirring paddle speed is 80 RPM, add two times the volume of deionized water to the silicon dioxide and wash repeatedly twice, remove the excess deionized water, and discharge;

[0029] A6, into the oven, 165℃, dry for 3 hours for standby, at this time, the particle size of silicon dioxide is between 15-25 nanometers;

[0030] A7, weigh a certain amount of silicon dioxide, pour it into a high-speed mixer, the temperature of the high-speed mixer is 120℃, the speed is 1200 RPM, weigh 5% of the mass of the silicon dioxide, dilute the vinyltriethoxysilane with anhydrous ethanol to 20% concentration for standby, use an atomizer to spray the diluted vinyltriethoxysilane into the high-speed mixer, continue to stir for 8 minutes, and 8 minutes of spraying is completed, discharge, place the silicon dioxide in a 120℃ oven for 6 hours, take it out for standby;

[0031] A8, place the silicon dioxide completed in step A7 in the rinsing pool, add 1.5 times the volume of anhydrous ethanol to the silicon dioxide, wash repeatedly three times, then add 2 times the volume of deionized water to the silicon dioxide, filter out the silicon dioxide, and place it in a 105℃ oven for drying for 5 hours;

[0032] B, preparation of modified material:

[0033] B1, put the PP recycled resin particles of single-cylinder washing machine inner barrel, photovoltaic film recycled particles, compatibilizer, black masterbatch into the stirring pot, then add wetting agent, 350 RPM, stir for 10 minutes;

[0034] B2, add processing aid package and treated silicon dioxide to the stirring pot, 350 RPM, stir for 10 minutes;

[0035] B3, add the mixed material to the main feeding loss weight scale;

[0036] B4, add chopped glass fiber to the side feeding loss weight scale at the sixth section of the extruder barrel;

[0037] B5, the equipment adopts 40:1 length-diameter ratio, the main loss-on-weighing scale is set to 35 kg / h, and the side loss-on-weighing scale is set to 15 kg / h;

[0038] B6, the main machine is started, the frequency is 38 Hz, the feeding is started, the auxiliary equipment is started, and the granulation production is carried out.

[0039] Further, in step A6, the particle size of the silicon dioxide is between 15-25 nanometers, which is measured by a laser nanoparticle size instrument, and the water absorption of the silicon dioxide is 4.7% of the self weight after 24 hours under the condition of 50% relative humidity and 23 DEG C.

[0040] Further, the silicon dioxide in step A8 is placed under the condition of 50% relative humidity and 23 DEG C for 24 hours, and the water absorption is less than or equal to 0.6% of the self weight.

[0041] Compared with the prior art, the present application has the following beneficial effects:

[0042] 1. The method uses single-cylinder washing machine inner barrel PP recycled granular resin (PCR) and photovoltaic film recycled granular resin recycled material, which greatly reduces the cost of the formula, and in addition, the use of recycled materials can reduce the dependence on virgin petrochemical products and reduce carbon emissions.

[0043] 2. The physical properties of the single-cylinder washing machine inner barrel PP recycled granular (PCR) are extremely similar to those of K7726H-RC (North Huajin), and the photovoltaic film recycled granular resin is a partially crosslinked material, which synergistically enhances the crosslinked part and the glass fiber when blended with the base material. The crosslinked molecular chain forms a three-dimensional network structure, which can still maintain good flexibility at low temperatures, avoiding material brittleness. In addition, the uncrosslinked part can act as an elastomer to toughen the base material.

[0044] 3. The treated silicon dioxide material has improved hydrophobicity, increasing compatibility with the base resin. During injection molding, the presence of treated silicon dioxide disrupts the directional arrangement of glass fibers, reducing the absolute value of the transverse and longitudinal shrinkage rate difference of the product, and further reducing the degree of product warpage. BRIEF DESCRIPTION OF DRAWINGS

[0045] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the following will briefly introduce the drawings needed in the embodiments. It should be understood that the following drawings only show some embodiments of the present application, and therefore should not be regarded as a limitation on the scope. For those skilled in the art, other related drawings can also be obtained without creative labor on the basis of these drawings.

[0046] Fig. 1 Preparation flow chart of high-strength, low-temperature-resistant and low-warp bottom guard plate material;

[0047] Fig. 2 Flow chart of the extraction and treatment process of silica. DETAILED DESCRIPTION

[0048] The application will be further described below in connection with the embodiments.

[0049] The application will be further described below in connection with the embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the application and are not intended to limit the scope of the application. In addition, it should be noted that, for the sake of brevity, only the parts of the drawings that are relevant to the application are shown in the drawings.

[0050] It should be noted that: similar signs and letters represent similar items in the following drawings, therefore, once an item is defined in one drawing, it does not need to be further defined and explained in subsequent drawings. At the same time, in the description of the application, the terms "first", "second" and the like are only used to distinguish the description and cannot be understood as indicating or implying relative importance.

[0051] The application provides a method for preparing a high-strength, low-temperature-resistant and low-warp bottom guard plate material, which meets the requirements of high strength, low temperature resistance and low warping at the same time. The treated silica is obtained after a series of reactions of by-products such as sodium silicate formed by manufacturing capacitor carbon from rice husk, the polypropylene material is single-cylinder washing machine inner barrel PP recycled material particles (PCR), the toughening agent is photovoltaic film recycled particles, and other materials are commercially available. The material achieves high strength effect through the cross-linking part of the glass fiber and the toughening agent, achieves low-temperature resistance through the uncross-linked part and the cross-linked part of the toughening agent, and reduces the difference between the transverse and longitudinal shrinkage of the product and the warping of the material by destroying the directional flow of the glass fiber through the treated silica during injection molding.

[0052] As shown in Figs. 1-2 A high-strength, low-temperature-resistant and low-warp bottom guard plate material and a preparation method thereof, comprising the following steps: weighing polypropylene resin particles, toughening agent resin particles, compatibilizer and black masterbatch into a stirring pot, then adding a wetting agent, stirring at 350 RPM for 10 minutes; adding a processing aid package and treated silica to the stirring pot, stirring at 350 RPM for 10 minutes, then adding the mixed material into a main feeder loss weight scale; using a 40:1 length-diameter ratio, adding chopped glass fiber into the side feeder loss weight scale at the sixth extruder cylinder, setting the discharge amount of the main loss weight scale to 35 kg / hour, and setting the discharge amount of the side loss weight scale to 15 kg / hour. Turn on the main machine, turn on the feeder, and turn on the auxiliary equipment to produce granules.

[0053] Further, the method specifically comprises the following steps:

[0054] Preparation of treated silica:

[0055] A. Processed silicon dioxide preparation:

[0056] A1, First, the by-product of sodium silicate formed by the production of rice hull capacitor carbon is filtered to remove impurities, and the concentration of sodium silicate in the test solution is tested;

[0057] A2, The sodium silicate solution is introduced into the evaporator, the evaporator is heated to boiling of the solution, the water in the by-product of sodium silicate is evaporated, and the concentration of sodium silicate is increased. When the concentration of sodium silicate reaches 20%-25%, stop heating and discharge;

[0058] A3, Enter the reaction tank, start the stirring paddle, the speed is 245 RPM, start the heating system, control the material temperature at 80-90℃, add 16% concentration hydrochloric acid through the additive pump, control the whole material PH value at 7.5-8.5, stop adding hydrochloric acid, at this time, the gel is generated (Na2SiO3+2HCI==2NaCI+H2SiO3↓), discharge;

[0059] A4, Enter the dehydration tank, heat to 152℃, until the weight of the material in the dehydration tank is constant, at this time, the gel is completely decomposed into silicon dioxide (H2SiO3= heating = H2O↑+SiO2↓), the water is discharged in the form of water vapor, and finally discharged;

[0060] A5, The material enters the rinsing tank, the stirring paddle speed is 80 RPM, and two times the volume of the deionized water is added for repeated cleaning twice, and the excess deionized water is discharged, and the material is discharged;

[0061] A6, Enter the oven, 165℃, dry for 3 hours for standby, at this time, the particle size of the silicon dioxide is between 15-25 nanometers;

[0062] A7, A certain amount of silicon dioxide is weighed and poured into a high-speed mixer, the temperature of the high-speed mixer is 120℃, and the speed is 1200 RPM. 5% of the mass of the silicon dioxide is weighed as vinyltriethoxysilane, and the vinyltriethoxysilane is diluted with anhydrous ethanol to a concentration of 20% for standby. The diluted vinyltriethoxysilane is sprayed into the high-speed mixer using an atomizer, and the stirring is continued for 8 minutes, and the spraying is completed at 8 minutes, and the material is discharged. The silicon dioxide is placed in a 120℃ oven and left still for 6 hours, and then taken out for standby;

[0063] A8, The silicon dioxide completed in step A7 is placed in a rinsing tank, 1.5 times the volume of the silicon dioxide is added as anhydrous ethanol, and the anhydrous ethanol is repeatedly cleaned three times (vinyltriethoxysilane is dissolved in ethanol), then 2 times the volume of the silicon dioxide is added as deionized water, and the silicon dioxide is filtered out and placed in a 105℃ oven for drying for 5 hours.

[0064] Further, the step A6, the silica particle size is between 15-25 nanometers, measured by laser nanoparticle size meter, the silica is placed in the relative humidity 50%, 23℃ conditions, 24 hours later, the water absorption amount reaches 4.7% of the weight.

[0065] Further, the step A6, the silica particle size is between 15-25 nanometers, measured by laser nanoparticle size meter, the silica is placed in the relative humidity 50%, 23℃ conditions, 24 hours later, the water absorption amount reaches 4.7% of the weight.

[0066] B, preparation of modified material:

[0067] B1, single cylinder washing machine inner barrel PP recycled material particle resin, photovoltaic film recycled particle resin, compatibilizer, black masterbatch is put into the stirring pot, then the wetting agent is added, 350 RPM, stirring for 10 minutes;

[0068] B2, processing aid package, treated silica is added to the stirring pot, 350 RPM, stirring for 10 minutes;

[0069] B3, the mixed material is added to the main feeding loss weight scale;

[0070] B4, the chopped glass fiber is added to the side feeding loss weight scale at the sixth section of the extruder barrel;

[0071] B5, the equipment adopts 40:1 length-diameter ratio, the discharge amount of the main loss weight scale is set to 35 kg / hour, and the discharge amount of the side loss weight scale is set to 15 kg / hour;

[0072] B6, start the main machine, the frequency is 38 Hz, start the feeding, start the auxiliary equipment, and carry out granulation production.

[0073] The high-strength, low-temperature-resistant and low-warp bottom guard plate material is made of the following weight parts of raw materials:

[0074] Polypropylene: 51 parts,

[0075] Toughening agent: 8 parts,

[0076] Compatibilizer: 5 parts,

[0077] Glass fiber: 30 parts,

[0078] Treated silica: 3 parts,

[0079] Processing aid package: 1 part,

[0080] Wetting agent: 0.5 parts,

[0081] Black masterbatch: 1.5 parts.

[0082] Further, the polypropylene is a single-cylinder washing machine inner barrel PP recycled material particle (PCR) with an ash content of 0.2% or less, which is commercially available; the toughening agent is a photovoltaic film, which is a thin film recycled particle made of four-carbon POE after partial crosslinking, and is commercially available.

[0083] Further, the compatibilizer is a granular polypropylene grafted maleic anhydride, and KT-1D product of Shenyang Ketong is selected.

[0084] Further, the glass fiber is T538G of Taishan Glass Fiber Co., Ltd., which is a chopped glass fiber, or 305B of Chongqing International Composite Material Co., Ltd., which is a chopped glass fiber.

[0085] Further, the silicon dioxide is a nano material in the form of powder, which is a by-product of sodium silicate formed by using rice husk to manufacture capacitive carbon, and is processed through steps A1-A6 to form a silicon dioxide powder, and then processed through steps A7-A8 to form a processed silicon dioxide. The by-products such as sodium silicate are provided by Jilin Kaiyu Biomass Development Co., Ltd.

[0086] Further, the processing aid package is a powder, which includes an antioxidant and a lubricant; wherein the antioxidant includes antioxidant 1010, antioxidant 3114, antioxidant 168, and antioxidant DSTDP, the content of antioxidant 1010 is 0.15%, the content of antioxidant 3114 is 0.15%, the content of antioxidant 168 is 0.2%, and the content of antioxidant DSTDP is 0.3%; the content of the lubricant EBS is 0.2%.

[0087] Further, the wetting agent is liquid No. 10 white oil.

[0088] Further, the black masterbatch is a PE carrier color masterbatch with a carbon black content of 35%, which is commercially available.

[0089] Comparative Example 1

[0090] 1. Put 51 parts of polypropylene, 8 parts of toughening agent, 5 parts of compatibilizer, and 1.5 parts of black masterbatch into a stirring pot, then add 0.5 parts of wetting agent, stir at 350 RPM for 10 minutes; wherein the polypropylene is K7726H-Beifang Huajin, the toughening agent is a photovoltaic film recycled particle, and the compatibilizer is KT-1D;

[0091] 2. Add 1 part of processing aid package and 3 parts of processed silicon dioxide to the stirring pot, stir at 350 RPM for 10 minutes;

[0092] 3. Put the mixed material into the main feeding loss weight scale;

[0093] 4. Add 30 parts of chopped glass fiber, specifically T538G, into the side feeding loss-in-weight scale at the sixth section of the extruder barrel;

[0094] 5. The equipment adopts a length-diameter ratio of 40:1, the feeding amount of the main loss-in-weight scale is set to 35 kg / hour, and the feeding amount of the side loss-in-weight scale is set to 15 kg / hour;

[0095] 6. Start the main machine, the frequency is 38 Hz, start the feeding, start the auxiliary equipment, and carry out granulation production.

[0096] Comparative Example 2

[0097] 1. Put 51 parts of polypropylene, 8 parts of toughening agent, 5 parts of compatibilizer, and 1.5 parts of black masterbatch into a stirring pot, then add 0.5 parts of wetting agent, stir at 350 RPM for 10 minutes; wherein the polypropylene is single-cylinder washing machine inner barrel PP recycled material particles (PCR), the toughening agent is HM7387-Tosoh Chemical, and the compatibilizer is KT-1D;

[0098] 2. Add 1 part of processing aid package and 3 parts of treated silicon dioxide to the stirring pot, stir at 350 RPM for 10 minutes;

[0099] 3. Add the mixed material into the main feeding loss-in-weight scale;

[0100] 4. Add 30 parts of chopped glass fiber, specifically T538G, into the side feeding loss-in-weight scale at the sixth section of the extruder barrel;

[0101] 5. The equipment adopts a length-diameter ratio of 40:1, the feeding amount of the main loss-in-weight scale is set to 35 kg / hour, and the feeding amount of the side loss-in-weight scale is set to 15 kg / hour;

[0102] 6. Start the main machine, the frequency is 38 Hz, start the feeding, start the auxiliary equipment, and carry out granulation production.

[0103] Comparative Example 3

[0104] 1. Put 51 parts of polypropylene, 8 parts of toughening agent, 5 parts of compatibilizer, and 1.5 parts of black masterbatch into a stirring pot, then add 0.5 parts of wetting agent, stir at 350 RPM for 10 minutes; wherein the polypropylene is single-cylinder washing machine inner barrel PP recycled material particles (PCR), the toughening agent is photovoltaic film recycled particles, and the compatibilizer is KT-1D;

[0105] 2. Silicon dioxide preparation:

[0106] 2-1. First, filter the by-products such as sodium silicate formed by rice husk manufacturing capacitor carbon, remove impurities, and test the concentration of sodium silicate in the solution;

[0107] 2-2, the sodium silicate solution is introduced into the evaporator, the evaporator is heated to boiling of the solution, the water in the by-products such as sodium silicate is evaporated, the concentration of sodium silicate is increased, when the concentration of sodium silicate reaches 20%-25%, the heating is stopped, and the material is discharged;

[0108] 2-3, entering the reaction pool, the stirring paddle is started, the rotating speed is 245 RPM, the heating system is started, the material temperature is controlled at 80-90 DEG C, 16% concentration hydrochloric acid is added through the additive pump, when the overall material PH value is controlled at 7.5-8.5, the addition of hydrochloric acid is stopped, at this time, the colloidal substance (Na2SiO3+2HCl==2NaCl+H2SiO3 down) is generated, and the material is discharged;

[0109] 2-4, entering the dehydration pool, the heating temperature is 152 DEG C, until the weight of the material in the dehydration pool is constant, at this time, the colloidal substance is completely decomposed into silicon dioxide (H2SiO3=heating=H2O up+SiO2 down), the water is discharged in the form of water vapor, and finally the material is discharged;

[0110] 2-5, the material enters the rinsing pool, the rotating speed of the stirring paddle is 80 RPM, two times of the volume of the silicon dioxide of deionized water is added repeatedly for two times of cleaning, the excess deionized water is discharged, and the material is discharged;

[0111] 2-6, entering the oven, 165 DEG C, drying for 3 hours for standby, at this time, the particle size of the silicon dioxide is between 15-25 nanometers;

[0112] 2-7, adding 1 part of processing aid package and 3 parts of 15-25 nanometer silicon dioxide into the stirring pot, 350 RPM, and stirring for 10 minutes;

[0113] 3, the mixed material is added into the main feeding loss weight scale;

[0114] 4, 30 parts of chopped glass fiber, specifically T538G, are added into the side feeding loss weight scale at the sixth section of the extruder barrel;

[0115] 5, the equipment adopts 40:1 length-diameter ratio, the discharge amount of the main loss weight scale is set to 35 kg / hour, and the discharge amount of the side loss weight scale is set to 15 kg / hour;

[0116] 6, the main machine is started, the frequency is 38 Hz, the feeding is started, the auxiliary equipment is started, and the granulation production is carried out.

[0117] Comparative Example 4

[0118] 1, 54 parts of polypropylene, 8 parts of toughening agent, 5 parts of compatibilizer, 1.5 parts of black masterbatch are put into the stirring pot, then 0.5 parts of wetting agent are added, 350 RPM, and stirring for 10 minutes; wherein the polypropylene is single-cylinder washing machine inner barrel PP regenerated material particles (PCR), the toughening agent is photovoltaic film regenerated particles, and the compatibilizer is KT-1D;

[0119] 2. Add 1 part of the processing aid package to the mixing bowl, stir at 350 RPM for 10 minutes;

[0120] 3. Add the mixed material to the main feeder loss weight scale;

[0121] 4. Add 30 parts of chopped glass fiber, specifically T538G, to the side feeder loss weight scale at the sixth section of the extruder barrel;

[0122] 5. The equipment has a length-diameter ratio of 40:1, and the discharge amount of the main loss weight scale is set to 35 kg / hour, and the discharge amount of the side loss weight scale is set to 15 kg / hour;

[0123] 6. Start the main machine with a frequency of 38 Hz, start the feeder, start the auxiliary equipment, and perform granulation production.

[0124] Example 1: Take 51 parts of polypropylene, 8 parts of toughening agent, 5 parts of compatibilizer, and 1.5 parts of black masterbatch, and put them into a mixing bowl. Then, add 0.5 parts of wetting agent, stir at 350 RPM for 10 minutes; wherein the polypropylene is single-cylinder washing machine inner barrel PP recycled material particles (PCR), the toughening agent is photovoltaic film recycled particles, and the compatibilizer is KT-1D.

[0125] 2. Preparation of treated silicon dioxide:

[0126] 2-1. First, filter the by-products such as sodium silicate formed by the rice hull manufacturing capacitor carbon, remove impurities, and test the concentration of sodium silicate in the solution;

[0127] 2-2. Introduce the sodium silicate solution into the evaporator, heat the evaporator to boiling of the solution, evaporate the water in the by-products such as sodium silicate, and increase the concentration of sodium silicate. When the concentration of sodium silicate reaches 20%-25%, stop heating and discharge;

[0128] 2-3. Enter the reaction tank, start the stirring paddle at 245 RPM, start the heating system, control the material temperature at 80-90℃, add 16% concentrated hydrochloric acid through the auxiliary pump, control the overall material PH value at 7.5-8.5, stop adding hydrochloric acid, at this time, generate a gel (Na2SiO3+2HCI==2NaCI+H2SiO3↓), and discharge;

[0129] 2-4. Enter the dehydration tank, heat to 152℃ until the weight of the material in the dehydration tank is constant, at this time, the gel is completely decomposed into silicon dioxide (H2SiO3= heating = H2O↑+SiO2↓), the water is discharged in the form of water vapor, and finally discharged;

[0130] 2-5. The material enters the rinsing tank, the stirring paddle rotates at 80 RPM, and two times the volume of the silicon dioxide of deionized water is added for repeated washing twice to remove excess deionized water, and then discharged.

[0131] 2-6, into the oven, 165℃, drying for 3 hours standby, at this time, the particle size of silica is between 15-25 nanometers;

[0132] 2-7, a certain amount of silica is weighed and poured into a high-speed mixer, the temperature of the high-speed mixer is 120℃, the speed is 1200 RPM, 5% of the mass of the silica is weighed as vinyl triethoxysilane, the vinyl triethoxysilane is diluted with anhydrous ethanol to a concentration of 20% for standby, the diluted vinyl triethoxysilane is sprayed into the high-speed mixer using an atomizer, and stirring is continued for 8 minutes, and the spraying is completed in 8 minutes, and the material is discharged, the silica is placed in a 120℃ oven for 6 hours, and then taken out for standby;

[0133] 2-8, the silica completed in step 2-step 7 is placed in a rinsing pool, 1.5 times the volume of the silica is added as anhydrous ethanol, and the rinsing is repeated three times (vinyl triethoxysilane is dissolved in ethanol), then 2 times the volume of the silica is added as deionized water, the silica is filtered out, and placed in a 105℃ oven for drying for 5 hours;

[0134] 2-9, 1 part of the processing aid package and 3 parts of the treated silica are added to a stirring pot, stirred at 350 RPM for 10 minutes;

[0135] 3, the mixed material is added to the main feeding loss weight scale;

[0136] 4, 30 parts of chopped glass fiber, specifically T538G, are added to the side feeding loss weight scale at the sixth section of the extruder barrel;

[0137] 5, the equipment adopts a length-diameter ratio of 40:1, the discharge amount of the main loss weight scale is set to 35 kg / hour, and the discharge amount of the side loss weight scale is set to 15 kg / hour;

[0138] 6, the main machine is started, the frequency is 38 Hz, the feeding is started, the auxiliary equipment is started, and the granulation production is carried out.

[0139] It should be particularly noted that, if a specific technology or condition is not specified in the examples, the technology or condition is carried out according to the description in the literature in the field or according to the product manual, and if the manufacturer of the reagent or instrument is not specified, it is a conventional product that can be obtained from the market.

[0140] The present application provides the component allocation ratio of Comparative Example 1-Comparative Example 4, the component allocation ratio of Comparative Example 1-Comparative Example 3 is shown in Table 1, in parts by weight:

[0141] Table 1

[0142]

[0143] The above test results are as follows: Table 2:

[0144] Table 2

[0145]

[0146] The reference standards are as follows:

[0147] Density: GB / T 1033.1, Tensile strength: GB / T 1040.2, Bending strength: GB / T 9341, Charpy notched impact strength: GB / T 1043.1, Shrinkage: GB / T 17037.4. Drop ball impact: three samples of 60mm x 60mm are cut from the relatively flat part of the product, and impact test is carried out. After the test, the appearance quality of the impact sample is visually inspected.

[0148] a. Room temperature, steel ball weight 500g ± 5g, drop ball height h = (300 ± 0.5) mm;

[0149] b. After cold resistance, the sample is placed in a super-low temperature box at a temperature of (-40 ± 2) ℃ for 24h, and immediately after taking out, impact is carried out, the steel ball weight is 500g ± 5g, and the drop ball height h = (400 ± 0.5) mm.

[0150] From Comparative Example 1 and Example 1: In this formula, the raw material K7726H (Beifang Huajin) is replaced by single-cylinder washing machine inner barrel PP recycled material particles (PCR) added to the formula, and the physical properties of the whole formula system are basically unchanged, which can achieve the purpose of cost reduction, carbon reduction and recycling.

[0151] From Comparative Example 2 and Example 1: Adding photovoltaic film recycled particles has more advantages than HM7387 (Dow Chemical), especially in bending strength, bending modulus, Charpy notched impact strength at -30℃, and drop ball impact at -40℃ for 24h.

[0152] From Comparative Example 3 and Example 1: The treated silicon dioxide is superior to the untreated silicon dioxide in terms of bending strength, bending modulus, and the absolute value of the difference between the transverse and longitudinal shrinkage.

[0153] From Comparative Example 3-Comparative Example 4 and Example 1: Adding untreated silicon dioxide has a lower absolute value of the difference between the transverse and longitudinal shrinkage than not adding silicon dioxide; adding treated silicon dioxide can greatly reduce the absolute value of the difference between the transverse and longitudinal shrinkage of the material, thereby reducing the warpage of the product.

[0154] In summary: In this formula, single-cylinder washing machine inner barrel PP recycled material particles (PCR) can be used to replace the raw material K7726H; photovoltaic film recycled particles have more advantages than HM7387 in terms of low temperature resistance and mechanical strength; silicon dioxide can reduce the absolute value of the difference between the transverse and longitudinal shrinkage of the material, and treated silicon dioxide has more advantages.

[0155] It is to be noted that the design of the digital prototype model, the parameter setting of each material, and the selection of the measurement plane are only the preferred embodiments of the present application and the principles of the technology applied. Those skilled in the art will understand that the present application is not limited to the specific embodiments described herein, and that various obvious changes, re-adjustments and substitutions can be made by those skilled in the art without departing from the scope of the present application. Therefore, although the present application has been described in detail through the above embodiments, the present application is not limited to the above embodiments, and can include more other equivalent embodiments without departing from the concept of the present application, and the scope of the present application is determined by the scope of the appended claims.

Claims

1. A high strength, low temperature resistant, low warpage floor pan material characterized in that, is made from the following raw materials by weight: Polypropylene: 51 parts, Toughening agent: 8 parts, Compatibilizer: 5 parts, Glass fiber: 30 parts, Treated silica: 3 parts, Processing aid package: 1 part, Wetting agent: 0.5 parts, Black masterbatch: 1.5 parts; The polypropylene is a single-cylinder washing machine inner barrel PP recycled material particle, with ash content below 0.2%; the toughening agent is a photovoltaic film recycled particle, which is a thin film made of four-carbon POE after partial crosslinking, and is made into a particle after recycling; the compatibilizer is a granular polypropylene grafted maleic anhydride; the wetting agent is a liquid 10# white oil; the black masterbatch is a PE carrier color masterbatch with carbon black content of 35%; The silica is a nanoscale material powder, which is a by-product of sodium silicate formed by manufacturing capacitor carbon from rice husk, and is finally formed into silica powder after treatment, and is treated to form treated silica.

2. A high strength, low temperature resistant, low warpage floor protection material according to claim 1, characterized in that: The glass fiber is a chopped glass fiber.

3. The high strength, low temperature resistant, low warpage floor protection material of claim 1, wherein: The processing aid package is a powder, including antioxidants and lubricants; wherein the antioxidants include antioxidant 1010, antioxidant 3114, antioxidant 168 and antioxidant DSTDP, the content of antioxidant 1010 is 0.15%, the content of antioxidant 3114 is 0.15%, the content of antioxidant 168 is 0.2%, and the content of antioxidant DSTDP is 0.3%; the content of lubricant EBS is 0.2%.

4. The method for preparing a high-strength, low-temperature resistant, and low-warpage bottom protective plate material according to claim 1, characterized in that, It includes the following steps: weigh the polypropylene resin particles, toughening agent resin particles, compatibilizer, and black masterbatch into a stirring pot; then, add the wetting agent, stir at 350 RPM for 10 minutes; then add the processing aid package and treated silica to the stirring pot, stir at 350 RPM for 10 minutes; add the mixed material to the main feeding loss weight scale; the equipment adopts a length-diameter ratio of 40:1, the chopped glass fiber is added to the side feeding loss weight scale at the sixth section of the extruder cylinder, the discharge amount of the main loss weight scale is set to 35 kg / hour, and the discharge amount of the side loss weight scale is set to 15 kg / hour; turn on the main machine, turn on the feeding, turn on the auxiliary equipment, and carry out the granulation production.

5. The method for preparing a high-strength, low-temperature resistant, and low-warpage bottom protection plate material according to claim 4, characterized in that, Specifically includes the following steps: A, preparation of treated silica: A1, first filter the by-product of sodium silicate formed by manufacturing capacitor carbon from rice husk to remove impurities, and test the concentration of sodium silicate in the solution; A2, introduce the sodium silicate solution into the evaporator, heat the evaporator to boiling of the solution, evaporate the water in the sodium silicate by-product, and increase the concentration of sodium silicate; when the concentration of sodium silicate reaches 20%-25%, stop heating and discharge; A3, enter the reaction tank, start the stirring paddle at 245 RPM, start the heating system, control the material temperature at 80-90℃, add 16% concentrated hydrochloric acid through the aid pump, control the overall material PH value at 7.5-8.5, stop adding hydrochloric acid, at this time, a gel is formed, and the discharge is completed; A4, enter the dehydration tank, heat to 152℃, until the weight of the material in the dehydration tank is constant, at this time, the gel is completely decomposed into silica, and the water is discharged in the form of water vapor, and finally the discharge is completed; A5, the material obtained in step A4 enters a rinsing pool, the stirring paddle rotates at 80 RPM, and two times the volume of the silica of deionized water is added repeatedly for two times of cleaning, the excess deionized water is discharged, and the material is discharged; A6, enter the oven, 165℃, dry for 3 hours for standby, at this time, the silica particle size is between 15-25 nanometers; A7, a certain amount of silica is weighed and poured into a high-speed mixer, the temperature of the high-speed mixer is 80℃, and the rotating speed is 1200 RPM, 5% of the mass of the silica of vinyl triethoxysilane is weighed, the vinyl triethoxysilane is diluted with anhydrous ethanol to a concentration of 20% for standby, the diluted vinyl triethoxysilane is sprayed into the high-speed mixer by using an atomizer, and stirring is continued for 8 minutes, and the spraying is completed at 8 minutes, the material is discharged, the silica is placed in an 80℃ oven for 6 hours, and taken out for standby; A8, the silica completed in step A7 is placed in a rinsing pool, 1.5 times the volume of the silica of anhydrous ethanol is added, and repeated cleaning is performed three times, 2 times the volume of the silica of deionized water is further added, the silica is filtered out, and is placed in a 105℃ oven for drying for 5 hours; B, preparation of modified material: B1, the PP recycled material granular resin in the single-cylinder washing machine inner barrel, the photovoltaic film recycled granular resin, the compatibilizer, and the black masterbatch are put into a stirring pot, and then the wetting agent is added, and stirring is performed at 350 RPM for 10 minutes; B2, the processing aid package and the treated silica are added to the stirring pot, and stirring is performed at 350 RPM for 10 minutes; B3, the mixed material is added to the main feeding loss weight scale; B4, the chopped glass fiber is added to the side feeding loss weight scale at the sixth extruder barrel; B5, the equipment adopts a length-diameter ratio of 40:1, the discharge amount of the main loss weight scale is set to 35 kg / hour, and the discharge amount of the side loss weight scale is set to 15 kg / hour; B6, the main machine is started, the frequency is 38 Hz, the feeding is started, the auxiliary equipment is started, and the granulation production is performed.

6. The method for preparing a high-strength, low-temperature resistant, and low-warpage bottom protection plate material according to claim 5, characterized in that: In step A6, the particle size of the silica is between 15-25 nanometers, which is measured by a laser nanoparticle size instrument, and after 24 hours under the condition of a relative humidity of 50% and a temperature of 23℃, the water absorption amount of the silica reaches 4.7% of the self-weight.

7. The method for preparing a high-strength, low-temperature resistant, and low-warpage bottom protection plate material according to claim 6, characterized in that: The silica in step A8 is placed under the condition of a relative humidity of 50% and a temperature of 23℃ for 24 hours, and the water absorption amount is ≤0.6% of the self-weight.

Citation Information

Patent Citations

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